CN108387959A - A kind of high acceleration test system cold light reflector of natural light aging and its plating method - Google Patents
A kind of high acceleration test system cold light reflector of natural light aging and its plating method Download PDFInfo
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- CN108387959A CN108387959A CN201810170109.8A CN201810170109A CN108387959A CN 108387959 A CN108387959 A CN 108387959A CN 201810170109 A CN201810170109 A CN 201810170109A CN 108387959 A CN108387959 A CN 108387959A
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- film
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- acceleration test
- cold light
- light reflector
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Classifications
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/08—Mirrors
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/10—Glass or silica
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/004—Investigating resistance of materials to the weather, to corrosion, or to light to light
Abstract
First of the present invention is designed to provide a kind of high acceleration test system cold light reflector of natural light aging, including plane quartz glass substrate and it is covered on the plane quartz glass substrate surface, the high refractive index film by two kinds of unlike materials and a kind of non-periodic multilayer that low refractive index film forms, it can reduce the loss of ultraviolet radiation reflection, reduce the degree of reflection of infrared light radiation simultaneously, to exclude influence of the infrared light radiation to the high accelerated test of light aging, the correlation of experimental result is improved.Second object of the present invention is to provide the plating method of the high acceleration test system cold light reflector of the natural light aging, this method degree of controllability height, it is ensured that the stabilization of cold light reflector optical property obtained.
Description
Technical field
The invention belongs to atmospherical exposure test fields, and in particular to a kind of high acceleration test system cold light of natural light aging
Speculum and its plating method.
Background technology
Atmospherical exposure test is a kind of Natural Environmental Test, it is that the product of non-packaging state is exposed to natural environment
In, it is directly subjected to the comprehensive function of factor of natural environment before the deadline, evaluates the environmental suitability of the product.
Although the real result of atmospherical exposure test is reliable, the general variation occurred in a natural environment or reflection are more
Slowly, it needs to be observed and recorded for a long time, generally some months or several years or even longer time, this greatly affected
Efficiency in practical application.Meanwhile the method that most situation uses simulating natural condition in the lab at present, instead of passing
The atmospherical exposure test of system.In the natural conditions simulation in laboratory, artificial simulated light is generally used to the simulation of illumination condition
The spectrum in source, this kind of manual simulation's light source generally has a certain difference between the spectrum of sunlight.The difference of these spectrum
It is very possible to eventually lead to experimental result inaccuracy, the especially difference of the cut off of ultraviolet spectra wavelength, it is likely that lead to light
The mechanism of aging changes, to make test result lose authenticity.
Therefore, in order to overcome above-mentioned technical problem, the high acceleration test system of natural light aging has been derived.This system
The condition provided and natural conditions are very close, while ensure that test result correlation, and can greatly shorten experiment
Period.However, there are still certain defects for the existing high acceleration test system of natural light aging：
The basic principle of the high acceleration test system of natural light aging is the effect by cold light reflector, by sun light reflection
It focuses, achievees the purpose that enhance optical radiation energy.Existing condenser mirror is typically employed in photovoltaic art, can reflect major part
Near-infrared radiation, but it is ultraviolet radioactive actually to influence light ager process.Infra-red radiation will produce fuel factor, influence sample
The effect of light aging test.Therefore the high acceleration test system of natural light aging needs to exclude infra-red radiation, and farthest anti-
Penetrate ultraviolet radioactive.
Invention content
First of the present invention is designed to provide a kind of high acceleration test system cold light reflector of natural light aging,
The loss of ultraviolet radiation reflection can be reduced, while reducing the degree of reflection of infrared light radiation, to exclude infrared light radiation pair
The influence of the high accelerated test of light aging, improves the correlation of experimental result.
Second object of the present invention is to provide the natural light aging high acceleration test system cold light reflector
Plating method, this method degree of controllability is high, it is ensured that the stabilization of cold light reflector optical property obtained.
The invention is realized by the following technical scheme：
A kind of high acceleration test system cold light reflector of natural light aging, including plane quartz glass substrate and covering
In what is formed on the plane quartz glass substrate surface, by the high refractive index film and a kind of low refractive index film of two kinds of unlike materials
The combination of non-periodic multilayer, the non-periodic multilayer is a (0.5H1L0.5H1)/b(0.5H2L0.5H2), wherein a, b
For periodic coefficient, H1、H2The high refractive index film of respectively two kinds unlike materials, L are low refractive index film.
The high acceleration test system cold light reflector of natural light aging of the present invention, by the quartz glass substrate
One layer of H is stacked on piece surface1, then it is sequentially stacked one layer of L, one layer of H1, it is alternately superimposed on a period, in last layer of H above-mentioned1
One layer of L, one layer of H are sequentially stacked on surface2, it is alternately superimposed on b period, until last layer of H2Film layer terminates.Through the above way
Obtained cold light reflector, optical property can meet making for the high acceleration test system of natural light aging well after stacked
With requiring.
Preferably, the periodic coefficient a of the non-periodic multilayer is 11~15, and periodic coefficient b is 8~11.
Preferably, the high refractive index film H1Coating materials use Ta2O5, high refractive index film H2Coating materials use TiO2, described
The coating materials of low refractive index film uses SiO2.By using high index film material Ta2O5、TiO2With low-refraction coating materials SiO2With this hair
Cold light reflector obtained, optical property can preferably reflect visible light and ultraviolet light, make visible after the bright mode is stacked
Light radiation and the loss of ultraviolet radioactive are preferably minimized, while can also further decrease the reflectivity of infrared light, to the maximum extent
Exclude influence of the infra-red radiation to test result.
Preferably, the H1Single layer thicknesses of layers be 16~66nm.
Preferably, the H2Single layer thicknesses of layers be 22~75nm.
Preferably, the single layer thicknesses of layers of the L is 38~180nm.
Most preferably, the non-periodic multilayer periodic coefficient a is 12, and periodic coefficient b is 10, the aperiodic multilayer
The overall thickness of totally 45 layers of film, film is 3034.33nm.
Other than the factor material used by the film layer for influencing optical property, the thickness of film layer is equally one extremely important
Index.The difference of thickness can cause the angle of reflection/refraction, the difference of efficiency, and for the different light radiation of wavelength, these are poor
It is different also different.Therefore the thickness for controlling each film layer is equally an important means for improving optical property.
A kind of plating method of the high acceleration test system cold light reflector of natural light aging, using e type electron gun evaporations
With ion source assisted technique, include the following steps：
(1) substrate cleaning cleans plane quartz glass substrate, removal quartz glass substrate surface using supersonic wave cleaning machine
Dust, polishing powder, mark etc.；
(2) installation Open ＆ Clean vacuum chamber, the high refraction of film layer order addition according to designed non-periodic multilayer
In rate coating materials and low-refraction coating materials to crucible, then quartz glass substrate is installed to spherical coating clamp, and installs
Modifying mask；
(3) it vacuumizes, heat and open vacuum pump vacuum chamber is vacuumized, while opening heating system, make vacuum chamber
Interior temperature is stablized at 210~230 DEG C always；
(4) ion source is opened when the vacuum degree in vacuum chamber reaches 4.0 × 10-3When Pa or more, turn-on flow rate meter is simultaneously filled with
Oxygen, while ion source is opened, quartz glass substrate surface is bombarded；
(5) plated film keeps the unlatching of vacuum pump and being filled with for oxygen, opens electron gun, and institute is pressed on quartz glass substrate surface
The film layer order alternating deposit plated film of the non-periodic multilayer of design, is monitored thicknesses of layers using film-thickness monitoring；
(6) after cooling is coated with, when vacuum chamber naturally cools to 95~105 DEG C, vacuum pump is closed, opens vacuum chamber
Door takes out cold light reflector；
(7) annealing by the cold light reflector of taking-up be put into 290~310 DEG C of high temperature oven constant temperature baking 1.5~
2.5 hours, film layer structure is made to recombinate, stress release.
Preferably, in step (5) H1And H2During being coated with of film layer, vacuum degree is not higher than 1.8 × 10-2Pa, with
Ensure that the microstructure of the high refractive index layer after the completion of being coated with can reach the requirement of plated film.
By the substrate cleaning of step (1), adhesive force of the non-periodic multilayer to quartz glass substrate can be effectively improved；
During the entire process of plated film, 210~230 DEG C of optical characteristics and mechanical property that can improve film layer are kept the temperature at.
Step (4) is bombarded using ion source, and the surface of quartz glass substrate can be made to be cleaned and be activated again, carried
Coefficient of concentration and adhesive force of the high film layer in substrate surface.
The entire process that is coated with of step (5) uses ion assisted deposition technology, so that film refractive index is increased, mechanical strength and
Hardness increases, environmental suitability is improved.
Compared with prior art, the invention has the advantages that：
1, the high acceleration test system cold light reflector of the natural light aging, by using a (0.5H1L0.5H1)/b
(0.5H2L0.5H2) non-periodic multilayer construction, realize visible light-near ultraviolet band high reflection, near infrared light low reflection
The reflectivity of function, more existing protection aluminium reflector visible light-near ultraviolet improves 3~5%, and it is especially close to enhance light radiation
Ultraviolet radioactive energy, while the more former protection aluminium reflector low 70% or more of reflectivity of near infrared band, effectively eliminate fuel factor
Influence to sample aging experiment improves the correlation of test result, has reached the high acceleration test system of luminescent radiation aging
Requirement；
2, the high acceleration test system cold light reflector of the natural light aging, using e types electron gun evaporation and ion
Source assisted deposition process is coated with, and the absorption of high index film material is on the one hand reduced, and so that multilayer film is obtained higher anti-
Rate is penetrated, so that multilayer film is obtained good mechanical performance and chemical stability, and then extend speculum service life,
Reduce damage of the daily maintenance to film layer simultaneously.
Description of the drawings
Fig. 1 is coated with schematic device for the high acceleration test system cold light reflector of natural light aging.
Fig. 2 is the structural schematic diagram of the high acceleration test system cold light reflector of natural light aging made from embodiment 1.
Fig. 3 is the reflectance spectrum of the high acceleration test system cold light reflector test of natural light aging made from embodiment 1
Curve graph.
Reference numeral：1- vacuum chambers；2- spherical shape coating clamps；3- modifying masks；4- electron guns；5- ion sources；6- quartz
Glass substrate；7-Ta2O5Film layer；8-SiO2Film layer；9-TiO2Film layer.
Specific implementation mode
The present invention is explained in detail below by specific embodiment：
Embodiment 1
The high acceleration test system of natural light aging is coated with cold light reflector through following steps：
(1) substrate cleaning removes the quartz glass substrate using supersonic wave cleaning machine cleaning plane quartz glass substrate 6
Dust, polishing powder, the mark on 6 surfaces etc.；
(2) installation Open ＆ Clean vacuum chamber 1, the film layer order addition according to the non-periodic multilayer designed by table -1 are high
In refractive index coating materials and low-refraction coating materials to crucible, then quartz glass substrate 6 is installed to spherical coating clamp 2, and
Modifying mask 3 is installed, the equipment after installation is as shown in Figure 1；
(3) it vacuumizes, heat and open vacuum pump vacuum chamber is vacuumized, while opening heating system, make vacuum chamber 1
Interior temperature is stablized at 220 DEG C always；
(4) ion source is opened when the vacuum degree in vacuum chamber reaches 4.0 × 10-3When Pa or more, turn-on flow rate meter is simultaneously filled with
Oxygen, while ion source 5 is opened, 6 surface of quartz glass substrate is bombarded；
(5) plated film keeps the unlatching of vacuum pump and being filled with for oxygen, opens electron gun 4, is pressed on 6 surface of quartz glass substrate
The film layer order alternating deposit plated film of non-periodic multilayer designed by table -1, is being coated with Ta2O5Film layer and TiO2When film layer, very
Reciprocal of duty cycle keeps being not higher than 1.8 × 10-2Pa is monitored thicknesses of layers using film-thickness monitoring；
(6) after cooling is coated with, when vacuum chamber 1 naturally cools to 100 DEG C or so, vacuum pump is closed, opens vacuum
The door of room 1 takes out cold light reflector；
(7) cold light reflector of taking-up is put into constant temperature in 300 DEG C of high temperature oven and toasted 2 hours by annealing, makes film
Layer structural rearrangement, stress release.
The structure for the high acceleration test system cold light reflector of natural light aging being coated with is as shown in Figure 2.To being coated with
The obtained high acceleration test system of natural light aging carries out reflectance spectrum test with cold light reflector, and the results are shown in Figure 3.From figure
3 as it can be seen that wavelength reflectivity of (include ultraviolet light and visible optical radiation) within the scope of 300~780nm is more than 90%, and wavelength
Then it is less than 10% in the reflectivity higher than 780nm (i.e. infrared light radiation).
Table -1
Embodiment 2
Difference lies in the non-periodic multilayer is as shown in following table -2 with embodiment 1 for embodiment 2.
Table -2
Embodiment 3
Difference lies in the non-periodic multilayer is as shown in following table -3 with embodiment 1 for embodiment 3.
Table -3
After tested, above-described embodiment 2 is reflected with the high acceleration test system of natural light aging obtained by embodiment 3 with cold light
Mirror structure and reflectance spectrum test are close with the result of embodiment 1.It should be pointed out that above-described embodiment is only intended to this
The content of invention is illustrated, rather than is limited, therefore appointing in the comparable meaning and scope with technical solution of the present invention
What changes, and is all considered as including within the scope of the present invention.
Claims (7)
1. a kind of high acceleration test system cold light reflector of natural light aging, which is characterized in that including plane quartz glass substrate
It piece and is covered on the plane quartz glass substrate surface, the high refractive index film by two kinds of unlike materials and a kind of low refraction
The combination of the non-periodic multilayer of rate film composition, the non-periodic multilayer is a（0.5H1L0.5H1）/b
（0.5H2L0.5H2）, wherein a, b is periodic coefficient, H1、H2The high refractive index film of respectively two kinds unlike materials, L are low refraction
Rate film.
2. the high acceleration test system cold light reflector of natural light aging according to claim 1, it is characterised in that described
The periodic coefficient a of non-periodic multilayer is 11~15, and periodic coefficient b is 8~11.
3. the high acceleration test system cold light reflector of natural light aging according to claim 1, which is characterized in that described
High refractive index film H1Coating materials use Ta2O5, high refractive index film H2Coating materials use TiO2, the coating materials use of the low refractive index film
SiO2。
4. the high acceleration test system cold light reflector of natural light aging according to claim 3, which is characterized in that described
H1Single layer thicknesses of layers be 16~66nm, the H2Single layer thicknesses of layers be 22~75nm, the single layer thicknesses of layers of the L
For 38~180nm.
5. the high acceleration test system cold light reflector of natural light aging according to claim 4, which is characterized in that described
Non-periodic multilayer periodic coefficient a be 12, periodic coefficient b is 10, and totally 45 layers of the non-periodic multilayer, the overall thickness of film is
3034.33nm。
6. the plating method of the high acceleration test system cold light reflector of Claims 1 to 5 any one of them natural light aging,
Using e types electron gun evaporation and ion source assisted technique, which is characterized in that include the following steps：
（1）Substrate cleaning cleans plane quartz glass substrate, the ash on removal quartz glass substrate surface using supersonic wave cleaning machine
Dirt, polishing powder, mark etc.；
（2）Installation Open ＆ Clean vacuum chamber, the film layer order according to designed non-periodic multilayer add high refractive index film
In material and low-refraction coating materials to crucible, then quartz glass substrate is installed to spherical coating clamp, and install amendment
Baffle；
（3）It vacuumizes, heat and open vacuum pump vacuum chamber is vacuumized, while opening heating system, keep vacuum indoor
Temperature is stablized at 210~230 DEG C always；
（4）Ion source is opened when the vacuum degree in vacuum chamber reaches 4.0 × 10-3When Pa or more, turn-on flow rate meter is simultaneously filled with oxygen
Gas, while ion source is opened, quartz glass substrate surface is bombarded；
（5）Plated film keeps the unlatching of vacuum pump and being filled with for oxygen, opens electron gun, on quartz glass substrate surface by set
The film layer order alternating deposit plated film of the non-periodic multilayer of meter, is monitored thicknesses of layers using film-thickness monitoring；
（6）After cooling is coated with, when vacuum chamber naturally cools to 95~105 DEG C, vacuum pump is closed, opens door for vacuum chamber,
Take out cold light reflector；
（7）The cold light reflector of taking-up is put into constant temperature baking 1.5~2.5 in 290~310 DEG C of high temperature oven by annealing
Hour, so that film layer structure is recombinated, stress release.
7. the plating method of the high acceleration test system cold light reflector of natural light aging according to claim 6, special
Sign is, in step（5）The H1And H2During being coated with of film layer, vacuum degree is not higher than 1.8 × 10-2Pa。
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| CN111041413A (en) * | 2019-12-11 | 2020-04-21 | 中国工程物理研究院激光聚变研究中心 | Method for improving surface shape precision of large-aperture reflector coating film |
| CN113151783A (en) * | 2021-03-02 | 2021-07-23 | 中国电器科学研究院股份有限公司 | Combined reflective film and preparation method thereof |
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| CN113151783A (en) * | 2021-03-02 | 2021-07-23 | 中国电器科学研究院股份有限公司 | Combined reflective film and preparation method thereof |
| CN113151783B (en) * | 2021-03-02 | 2022-04-19 | 中国电器科学研究院股份有限公司 | Combined reflective film and preparation method thereof |
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